ABSTRACT This study presents an efficient approach for the separation and preconcentration of norepinephrine (NOR) from pharmaceutical formulations, environmental water, and human urine samples using a dispersive micro – solid phase extraction (DμSPE) technique employing magnetic nanoadsorbents. Two adsorbents, Fe3O4@TTAB and Fe3 O4@SiO2@TTAB, were prepared by functionalising iron oxide and silicacoated iron oxide nanoparticles with the cationic surfactant tetradecyltrimethylammonium bromide (TTAB). NOR was first converted into a sensitive diazonium dye via reaction with diazotised sulphamethazine and then extracted using mixed ademicelle – hemimicelle magnetic solid-phase extraction, followed by spectrophotometric quantification. Key adsorption parameters, including contact time, adsorbent dosage, solution pH, and reagent concentration, were optimised to elucidate the dye adsorption mechanism, and sorbent reusability was evaluated over six adsorption – desorption cycles. The surfactant-coated nanoparticles provided high extraction efficiencies, achieving preconcentration factors of 35 for Fe3O4@TTAB and 56 for Fe3O4@SiO2@TTAB, with recoveries of 96–102% and relative standard deviations below 3% for both adsorbents. The method displayed linearity ranges of 0.1–6.0 μg/mL for Fe3O4@TTAB and 0.05–6.0 μg/ mL for Fe3O4@SiO2@TTAB, with detection limits of 0.035 and 0.019 μg/mL, respectively. These results confirm that DμSPE is a reliable and sustainable approach for NOR extraction and preconcentration from diverse matrices.
A new spectrophotometric method has been developed for the assay of olanzapine (OLN.) in pure and dosage forms. The method is based on the diazocoupling of (OLN.) with diazotized p-nitroaniline in alkaline medium to form a stable brown colored water-soluble azo dye with a maximum absorption at 405 nm. The variables that affect the completion of reaction have been carefully optimized. Beer’s law is obeyed over the concentration range of (0.5-45.0 μg.mL-1) with a molar absorptivity of 1.5777×104 L.mol-1.cm-1. The limit of detection was 0.3148 μg.mL-1 and Sandell’s sensitivity value was 0.0198 μg.cm-2. The propose
... Show MoreDoxycycline hyclate is an antibiotic drug with a broad‐spectrum activity against a variety of gram‐positive and gram‐negative bacteria and is frequently used as a pharmacological agent and as an effector molecule in an inducible gene expression system. A sensitive, reliable and fast spectrophotometric method for the determination of doxycycline hyclate in pure and pharmaceutical formulations has been developed using flow injection analysis (FIA) and batch procedures. The proposed method is based on the reaction between the chromogenic reagent (V4+) and doxycycline hyclate in a neutral medium, resulting in the formation of a yellow compound that shows maximum absorbance at 3
This study was aimed to synthesis Ag2O nanoparticles (N.P.s) utilizing the Ginger plant (Zingiber officinale) extract. As catalysts for pyran derivatives formation employing a three-component coupling reaction among aromatic and aliphatic aldehydes, malononitrile, and dimedone. The nanoparticles exhibit robust catalytic activity with high productivity. Results revealed that Ag2O NPs improved various vital features, like higher yields, reaction time, simple chemical separation, catalytic economic efficiency, and quick process. This study aimed to cyclize heterocyclic compounds to provide new hetero compounds applying nano-oxides obtained from natural (unmanufactured) sources and used in several medical, pharmaceutical, and industrial
... Show MoreMetal nanoparticles can serve as an efficient nano-heat source with confinement photothermal effects. Thermo-plasmonic technology allows researchers to control the temperature at a nanoscale due to the possibility of precise light propagation. The response of opto-thermal generation of single gold-silica core-shell nanoparticle immersed in water and Poly-vinylpyrrolidone surrounding media is theoretically investigated. Two lasers (CW and fs pulses) at the plasmonic resonance (532 nm) are utilized. For this purpose, finite element method is used via COMSOL multiphysics to find a numerical computation of absorption cross section for the proposed core –shell NP in different media. Thermo-plasmonic response for both lasers is studied. The
... Show MoreCharge transfer complex formation method has been applied for the spectrophotometric determination of erythromycin ethylsuccinate, in bulk sample and dosage form. The method was accurate, simple, rapid, inexpensive and sensitive depending on the formed charge- transfer complex between cited drug and, 2,3- Dichloro-5,6-dicyano-p- benzoquinone (DDQ) as a chromogenic reagent. The formed complex shows absorbance maxima at 587 nm against reagent blank. The calibration graph is linear in the ranges of (10 - 110) μg.mL-1 with detection limit of 0.351μg.mL-1. The results show the absence of interferences from the excipients on the determination of the drug. Therefore the proposed method has been successfully applied for the determination of eryth
... Show MoreBased on the diazotization-coupling reaction, a new, simple, and sensitive spectrophotometric method for determining of a trace amount of (BPF) is presented in this paper. Diazotized metoclopramide reagent react with bisphenol F produces an orange azo-compound with a maximum absorbance at 461 nm in alkaline solution. The experimental parameters were optimized such as type of alkaline medium, concentration of NaOH, diazotized metoclopramide amount, order additions, reaction time, temperature, and effect of organic solvents to achieve the optimal performance for the proposed method. The absorbance increased linearly with increasing bisphenol F concentration in the range of 0.5-10 μg mL-1 under ideal conditions, with a correlati
... Show MoreThe prepared nanostructure SiO2 thin films were densified by two techniques (conventional and Diode Pumped Solid State Laser (DPSS) (532 nm). X-ray diffraction (XRD), Field Emission Scanning electron microscopy (FESEM), and Atomic Force Microscope (AFM) technique were used to analyze the samples. XRD results showed that the structure of SiO2 thin films was amorphous for both Oven and Laser densification. FESEM and AFM images revealed that the shape of nano silica is spherical and the particle size is in nano range. The small particle size of SiO2 thin film densified by DPSS Laser was (26 nm) , while the smallest particle size of SiO2 thin film densified by Oven was (111 nm).
A simple and rapid high performance liquid chromatographic with fluorescence detection method for the determination of the aflatoxin B1, B2, G1 and G2 in peanuts, rice and chilli was developed. The sample was extracted using acetonitrile:water (90:10, v/v%) and then purified by using ISOLUTE multimode solid phase extraction. After the pre-column derivatisation, the analytes were separated within 3.7 min using Chromolith performance RP-18e (100–4.6 mm) monolithic column. To assess the possible effects of endogenous components in the food items, matrix-matched calibration was used for the quantification and validation. The recoveries of aflatoxins that were spiked into food samples were 86.38–104.5% and RSDs were <4.4%. The method was
... Show MoreAn accurate and sensitive spectrophotometric method has been developed for the determination of carbamazepine (CRN.) in pure and dosage forms. The method is based on the oxidation of 2,4-dinitrophenylhydrazine (2,4-DNPHz) by potassium periodate than coupling with carbamazepine (CRN.) in alkaline medium to form a stable yellowish brown colored water-soluble dye with a maximum absorption at 485 nm. The variables that affect the completion of reaction have been carefully optimized. Beer’s law is obeyed over the concentration range of (4-50 μg.mL-1) with molar absorptivity of (6.7335×103 L.mol-1.cm1). The limit of detection was (0.1052 μg.mL-1) and Sandell’s sensitivity value was 0.0350 μg.cm-2.
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